Sunde-Brown Peter, Miller Gavin J, Houston Todd A
Institute for Glycomics, Griffith University, Gold Coast Campus, Southport 4215 , Queensland, Australia.
School of Chemical and Physical Sciences and Centre for Glycoscience, Keele University, Keele, Staffordshire ST5 5BG, U.K.
J Org Chem. 2025 Feb 14;90(6):2288-2297. doi: 10.1021/acs.joc.4c02667. Epub 2025 Feb 5.
We report a practical 5 g scale stereoselective synthesis of the valuable iminosugar DMDP from d-fructose in only 7 synthetic steps and in a 70% overall yield, which doubles previously reported yields. This process requires only two chromatographic purification steps, taking advantage of a regioselective Appel reaction. The regioselective reaction has also been applied on a similar scale to prepare the C-2 diastereomer of DMDP, DGDP, from l-sorbose in 7 steps (two purifications) and 56% overall yield, albeit with diminished diastereomeric purity (d.r. 90:10). The C-5 regioselectivity has also been illustrated on d-psicose and d-tagatose, making this an attractive method for preparing pyrrolidine iminosugars or 5-thiosugars from ketopyranoses.
我们报道了一种实用的5克规模的立体选择性合成方法,以d-果糖为原料,仅通过7步合成即可得到有价值的亚氨基糖DMDP,总产率为70%,是此前报道产率的两倍。该过程仅需两步柱色谱纯化,利用了区域选择性Appel反应。该区域选择性反应也已应用于类似规模的反应,以l-山梨糖为原料,通过7步反应(两步纯化)制备DMDP的C-2非对映异构体DGDP,总产率为56%,尽管非对映体纯度有所降低(d.r. 90:10)。C-5区域选择性也已在d-阿洛酮糖和d-塔格糖上得到证实,这使得该方法成为从酮吡喃糖制备吡咯烷亚氨基糖或5-硫代糖的一种有吸引力的方法。